US6143073A - Methods and apparatus for minimizing white point defects in quartz glass crucibles - Google Patents

Methods and apparatus for minimizing white point defects in quartz glass crucibles Download PDF

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Publication number
US6143073A
US6143073A US09/195,886 US19588698A US6143073A US 6143073 A US6143073 A US 6143073A US 19588698 A US19588698 A US 19588698A US 6143073 A US6143073 A US 6143073A
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Prior art keywords
electrodes
crucible
silica
reactive gas
electrode
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US09/195,886
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English (en)
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Marc A. Christman
Robert O. Mosier
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Shin Etsu Quartz Products Co Ltd
Heraeus Shin Etsu America Inc
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Heraeus Shin Etsu America Inc
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Priority to US09/195,886 priority Critical patent/US6143073A/en
Assigned to HERAEUS SHIN-ETSU AMERICA reassignment HERAEUS SHIN-ETSU AMERICA ASSIGNMENT OF ASSIGNORS INTEREST (SEE DOCUMENT FOR DETAILS). Assignors: MOSIER, ROBERT O., CHRISTMAN, MARC A.
Priority to EP99122937A priority patent/EP1002770A3/de
Priority to PCT/US1999/027624 priority patent/WO2000029648A1/en
Priority to JP2000582623A priority patent/JP4416952B2/ja
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Publication of US6143073A publication Critical patent/US6143073A/en
Assigned to SHIN-ETSU QUARTZ PRODUCTS CO., LTD. reassignment SHIN-ETSU QUARTZ PRODUCTS CO., LTD. ASSIGNMENT OF ASSIGNORS INTEREST (SEE DOCUMENT FOR DETAILS). Assignors: HERAESUS SHIN-ETSU AMERICA, INC.
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    • C—CHEMISTRY; METALLURGY
    • C03—GLASS; MINERAL OR SLAG WOOL
    • C03B—MANUFACTURE, SHAPING, OR SUPPLEMENTARY PROCESSES
    • C03B19/00—Other methods of shaping glass
    • C03B19/09—Other methods of shaping glass by fusing powdered glass in a shaping mould
    • C03B19/095—Other methods of shaping glass by fusing powdered glass in a shaping mould by centrifuging, e.g. arc discharge in rotating mould
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
    • Y02P40/00—Technologies relating to the processing of minerals
    • Y02P40/50—Glass production, e.g. reusing waste heat during processing or shaping
    • Y02P40/57—Improving the yield, e-g- reduction of reject rates
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y10—TECHNICAL SUBJECTS COVERED BY FORMER USPC
    • Y10S—TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y10S117/00—Single-crystal, oriented-crystal, and epitaxy growth processes; non-coating apparatus therefor
    • Y10S117/90—Apparatus characterized by composition or treatment thereof, e.g. surface finish, surface coating
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y10—TECHNICAL SUBJECTS COVERED BY FORMER USPC
    • Y10T—TECHNICAL SUBJECTS COVERED BY FORMER US CLASSIFICATION
    • Y10T117/00—Single-crystal, oriented-crystal, and epitaxy growth processes; non-coating apparatus therefor
    • Y10T117/10—Apparatus
    • Y10T117/1024—Apparatus for crystallization from liquid or supercritical state
    • Y10T117/1032—Seed pulling

Definitions

  • the present invention generally relates to crucible fabrication. Specifically, the present invention relates to methods and apparatus for making quartz glass crucibles that are suitable for use in pulling silicon single crystals for semiconductor applications.
  • CZ Czochralski
  • a crucible is one vessel commonly employed in this pulling operation for making ingots of silicon single crystals.
  • Crucibles are typically configured in a bowl shape, with walls and a bottom, to contain the molten silicon during the pulling operation.
  • Crucibles may be made of any material which adequately contains the molten silicon without contaminating it, yet introduces a desired amount of oxygen into the molten silicon.
  • One of the most widely used materials for such crucibles is silica or quartz glass.
  • Quartz glass crucibles can be manufactured by many processes.
  • a blade is used to scrape the particles to obtain a desired shape and, when needed, remove excess particles. Heat is applied to melt and fuse the silica or quartz particles, thus forming the wall and bottom of the crucible. After cooling, the crucible is removed from the mold.
  • crucible walls are opaque because they contain numerous tiny bubbles. When the bubbles open during the crystal-pulling operation, it can damage the silicon ingots.
  • an inner layer is often formed on the inside of the crucible.
  • quartz particles are formed into a crucible shape in a rotating mold by fusing the particles with an electric arc near the center of the rotating axis.
  • the silica or quartz particles are introduced through the arc created between opposing electrodes, often made of graphite. In passing through the arc, the particles are substantially--if not completely--melted. Heating the silica particles using the arc, however, causes a substantial quantity of silica vapor to form.
  • the silica vapor condenses on any object whose surface temperature is lower than the silica vapor, such as the cooler portions of the electrodes, and becomes silica particles.
  • the graphite electrodes erode during the crucible-making process due to oxidation of the graphite, the silica particles condensed on the electrodes fall away in flakes.
  • the present invention provides methods and apparatus for manufacturing silica crucibles containing few, if any, white point defects.
  • the white point defects are reduced during the inventive process by decreasing the amount of silica vapor condensing on electrodes used in the manufacturing process.
  • the silica vapor condensation is decreased by providing a flow of a protective or non-reactive gas or gas mixture over areas of the graphite electrodes where the silica vapor might condense.
  • the flow of protective gas or gas mixture is provided by nozzles, jets, or the like located proximate the desired areas of the electrodes.
  • the present invention includes a method for making at least one silica crucible which comprises providing a crucible substrate, providing a plurality of electrodes having an arc or plasma discharge therebetween, melting silica particles by introducing them through the arc or plasma discharge toward the crucible substrate, protecting the electrodes from silica vapor condensation, and cooling the crucible to its final form.
  • the plurality of electrodes can be graphite electrodes and the arc discharge established by voltage across the electrodes.
  • the electrodes are protected by flowing a non-reactive gas or mixture of non-reactive gases over a desired portion of the electrodes to reduce the amount of silicon oxide vapor condensing on the electrodes.
  • the non-reactive gas may be neon, helium, argon, or nitrogen.
  • the method reduces the amount of white point defects in a plurality of crucibles so that less than 7% of the crucibles contain is white point defects.
  • the present invention also includes an apparatus for making a silica crucible which comprises a crucible substrate, a plurality of electrodes having an arc or plasma discharge therebetween, means for introducing silica particles through the arc or plasma discharge and into the crucible substrate, and means for protecting at least a portion of the electrodes from silica vapor condensation.
  • the electrodes can be graphite electrodes and the arc discharge established by voltage through the electrodes.
  • the protecting means includes flowing means for establishing a flow of a non-reactive gas or mixture of non-reactive gases over the desired portion of the electrodes.
  • the flowing means may be at least one nozzle proximate the desired portion of the electrode.
  • FIGS. 1-3 are views of one process and apparatus for making quartz glass crucibles according to the present invention.
  • FIGS. 1-3 presented in conjunction with this description are views of only particular portions--rather than complete portions--of a quartz glass crucible and an apparatus for making the same.
  • FIG. 1 illustrates an exemplary crucible making-process in which the present invention can be employed.
  • rotatable mold 10 is provided with rotating shaft 21.
  • Electrodes 4, 5, and 6 are disposed within mold 10 and are held by electrode holders 1, 2, and 3, respectively, which typically are metallic double-walled pipe cooled with water between the walls.
  • Grain supply means 7 supplies quartz or silica particles (or powder or grain) 8 near the electrodes and into mold 10 to form a bubble-free layer on the inner surface of the quartz glass crucible 9.
  • Protecting devices 11, 12, and 13 are attached to electrode holders 1, 2, and 3, respectively.
  • mold 10 depends on the desired configuration and size of crucible 9 to be produced. Mold 10 may be made of any suitable material having a satisfactory heat resistance and mechanical strength, yet which may be formed into any desired configuration, such as stainless steel or graphite.
  • Crucible 9 is formed on the inner surface of mold 10 by any suitable process.
  • mold 10 is rotated about rotating shaft 21.
  • High-purity silicon dioxide grain 8 is then supplied near electrodes 4, 5, and 6, and directed toward the inner surface of mold 10.
  • an arc discharge is produced across the electrodes, some quartz grain--if not all--is melted by the arc.
  • the grain is simultaneously deposited on the inner surface of mold 10 to form a substantially bubble-free quartz glass layer of a predetermined thickness depending on the total fusion time.
  • Electrodes 4, 5, and 6 are made of any suitable material, such as carbon or graphite.
  • the electrodes are connected to water-cooled metallic electrode holders as shown in FIG. 1, with a diameter 85% to 150% of that of the electrode, at the end thereof to cool the electrodes with water.
  • the arc discharge may be of a bulged configuration so that when grain 8 passes through, it is distributed throughout a wide range of the inner surface of mold 10.
  • silica vapor or fume is released and condenses on the electrodes, especially on the cooler portions of the electrodes, including the areas near the water-cooled end of the electrode. Accordingly, silica vapor deposition is heaviest at the cooler portions of the electrodes. As discussed above, this causes "white point” defects in the crucible since the condensed silica can "flake off” the electrodes during the manufacturing process.
  • the present invention includes means for reducing the condensation of silicon dioxide vapor on the graphite electrodes, thus reducing these white point defects.
  • the means for reducing this silica vapor condensation on the electrodes includes an apparatus which blows a protecting or non-reactive gas or gas mixture over a portion of the electrodes. Any suitable flow of protecting gas across the surface of the graphite electrode can be employed in the present invention, provided it lifts the silica vapor away from the electrode and/or reduces the amount of silica vapor condensing on the electrodes.
  • Silica fume deposition may not be uniform about the circumference of the electrode.
  • the side of the electrode facing away from the other electrode(s)--being the most cool-- is where the most silica deposits. Thus, the flow of the protecting gas can be concentrated there.
  • the silica vapor By keeping the silica vapor away from the graphite electrode, the vapor is prevented from condensing on the graphite electrode. Instead, the silica vapor is exhausted and/or condenses on a more stable surface which holds the condensed silica vapor until the crucible is formed. Accordingly, the silica vapor does not "flake off" the electrodes and create white point defects in the crucible.
  • Any suitable gas (or mixture of gases) which protects the electrodes from the silica vapor and/or does not react with the quartz glass crucible, silica powder, and the electrodes can be employed in the present invention.
  • gases include, but are not limited to, neon (Ne), helium (He), argon (Ar), nitrogen (N 2 ), and mixtures thereof.
  • substantially pure nitrogen is employed as the non-reactive gas in the present invention.
  • Nitrogen is the preferable gas because of its reasonable cost and minimal interference with the arc characteristics.
  • any apparatus suitable for blowing the non-reactive gas across the surface of the electrodes can be employed in the present invention.
  • One such apparatus is illustrated in FIG. 2, where the non-reactive gas is blown past electrodes 4, 5, and 6 by protecting devices 11, 12, and 13.
  • Protecting devices 11, 12, and 13 generally comprise blowing means for providing a flow of the non-reactive gas, supplying means for supplying the non-reactive gas to the blowing means, and controlling means for regulating the flow of the protective gas.
  • Protecting devices 11, 12, and 13 should be located near the respective electrode so a proper flow of non-reactive gas is established. In the embodiment illustrated in FIG. 2, protecting devices 11, 12, and 13 may be fixed to the electrode holder by fixture means 18.
  • the blowing means of protecting devices 11, 12, and 13 may be at least one conventional nozzle, including a ring of pipe or hollow double-wall casing with a sealed end which is equipped with an array of downward-facing holes 17 spaced around the electrode holder to direct a stream of gas along the electrode surface.
  • the nozzle(s) preferably should be a line source or array of discrete sources. The nozzle(s) should be attached to the electrode holders, rather than the electrodes, to prevent overheating of the nozzle(s).
  • the nozzles have a configuration (e.g., ring) and outside circumference consistent with the configuration and circumference of the electrode encompassed.
  • the diameter of the nozzle/hole array may range from about 110% to about 200% of the outer diameter of the electrode holder, and is preferably about 130% of the outer diameter of the electrode holder.
  • the number and size of holes, as well as the spacing, will depend on the desired flow characteristics. For example, given a cathode diameter of 35 mm and an anode diameter of 60 mm, the anode rings have 20 holes with a 1/32" diameter and the cathode rings have 18 holes with a 1/16" diameter.
  • the distance between any hole (or nozzle) is less than twice the distance between the hole and the electrode surface.
  • the length and array of the nozzles can be adjusted to deliver the gas flow to the area of highest fume build up.
  • the holes on the center electrode nozzle ring should be arranged uniformly around the circumference of the electrode since the silica fume is deposited uniformly.
  • the fume deposition is not uniform.
  • the heaviest fume deposits on the outer side of the electrode opposite the center electrode. Therefore, the blow holes are more dense in this area.
  • blowing means include other types of nozzles, jets, and the like which could establish the desired flow of protecting gas.
  • Blowing means can have other shapes and configurations (e.g., rectangular) depending on the shape and configuration of the electrodes.
  • the supplying means should be properly connected to the blowing means to insure sufficient flow of protective gas.
  • supply tubes 14, 15, and 16 can be mounted in any desired configuration to protecting devices 11, 12, and 13, respectively.
  • the supplying means is also connected to storage means (not shown), such as a reservoir, containing the non-reactive gas.
  • the supplying means and blowing means can be made of the same or different material. Suitable materials include those materials which do not introduce impurities or degrade the crucible making process, such as high-purity quartz glass, sapphire, diamond, or zirconia. Preferably, the blowing and supplying means are constructed of high-purity silica or quartz glass.
  • Controlling means are located between the storage means and the blowing means to control the flow rate of the non-reactive gas. Controlling means are required to properly control the flow rate of the non-reactive gas.
  • the total gas flow though the nozzle array can range from about 80 cm 3 /sec, which can be employed while fusing the crucible substrate, to about 10,000 cm 3 /sec, which can be employed when introducing silica particles through the arc. Less than about 80 cm 3 /sec, and more specifically less than 0.4 cfm (cubic feet per minute) when nitrogen is the non-reactive gas, can be ineffective in reducing build up of the silica vapor and ineffective in protecting the nozzle from heat damage.
  • the non-reactive gas can interfere with the arc by essentially blowing away the ionized gases which provide the conductive path for the arc, thus requiring additional voltage to re-ionize the path between the electrode to maintain the arc.
  • the nitrogen gas flow should also be controlled within the desired flow rate in order to minimize disruption of the arc. Disrupting the arc can cause premature erosion of the electrode, stoppage or sputtering of the arc, changes in the crucible dimension, and bubble formation on the inner surface of the crucible.
  • the flow rate of the non-reactive gas should also be controlled to proportionately respond to the condensation rate of the silica vapor. As the amount of the silica vapor increases or decreases, there should be a corresponding increase or decrease in the flow rate of the non-reactive gas past the electrodes to lift the silica vapor away from the electrodes.
  • the flow rate of the non-reactive gas near the electrodes can be optionally pulsed. Pulsation reduces the total arc disruption over time while maintaining the desired non-reactive gas flow to suppress the condensation of silica on the electrodes.
  • the gas flow rate and pulsing of the gas is maintained either manually via a pressure regulator, needle valves, and flow gauges or automatically via a mass flow controller, programmable logic controller, and a series of pneumatic solenoids.
  • Protecting devices 11, 12, and 13 can be located at any desired position of the electrode holder and/or the electrode. Generally, protecting devices 11, 12, and 13 are located where they can reduce--and preferably prevent--silica vapor deposits. Preferably, the protecting devices are located proximate to the areas of the electrodes where the silica vapor deposits the most, such as the cooler parts of the electrodes.
  • Illustrations (1), (2), and (3) of FIG. 3 depict some of the various locations of protecting device 12 attached to the center electrode holder 2 in the present invention.
  • Illustration (4) of FIG. 3 represents an electrode with no protective device attached to reduce the amount of silica vapor deposits. Without a protecting device, fume or silica vapor deposits 19 on the upper part of the electrode, forms a film, and then flakes off.
  • gas blown from holes 17 sweeps down the electrode holder surface and then along the electrode surface.
  • the distance between the nozzle array and the end of the electrode holder should be optimized, and is preferably up to about three times the diameter of the electrode holder.
  • This configuration minimizes silica vapor deposits 19 on the electrode, but the nozzle can be quickly damaged by the plasma heat. Accordingly, the nozzle array should not be located too near the electrodes, at least when using materials that are easily damaged by the plasma heat.
  • Using the protecting gas or gas mixture according to the present invention greatly decreases the white point defects in crucibles.
  • a batch of crucibles can be manufactured with losses less than the normal loss rate for white point defects, which typically run about 7%.
  • a batch of 63 crucibles were manufactured with no to about less than 2% losses due to white point defects.

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  • Engineering & Computer Science (AREA)
  • Chemical & Material Sciences (AREA)
  • Manufacturing & Machinery (AREA)
  • Materials Engineering (AREA)
  • Organic Chemistry (AREA)
  • Crystals, And After-Treatments Of Crystals (AREA)
  • Glass Melting And Manufacturing (AREA)
US09/195,886 1998-11-19 1998-11-19 Methods and apparatus for minimizing white point defects in quartz glass crucibles Expired - Lifetime US6143073A (en)

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Application Number Priority Date Filing Date Title
US09/195,886 US6143073A (en) 1998-11-19 1998-11-19 Methods and apparatus for minimizing white point defects in quartz glass crucibles
EP99122937A EP1002770A3 (de) 1998-11-19 1999-11-18 Verfahren und Vorrichtung zur Minimalisierung von Weissfleckenfehlern in Quartzglastöpfen
PCT/US1999/027624 WO2000029648A1 (en) 1998-11-19 1999-11-19 Methods and apparatus for minimizing white point defects in quartz glass crucibles
JP2000582623A JP4416952B2 (ja) 1998-11-19 1999-11-19 石英ガラスるつぼの白点欠陥を最小限にする方法及び装置

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WO (1) WO2000029648A1 (de)

Cited By (13)

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Publication number Priority date Publication date Assignee Title
US20020083741A1 (en) * 2000-12-29 2002-07-04 Pandelisev Kiril A. Hot substrate deposition of fused silica
US20020139143A1 (en) * 2001-03-08 2002-10-03 Gabriele Korus Method of producing a quartz glass crucible
US20020170316A1 (en) * 2000-07-11 2002-11-21 Johann Leist Method and device for producing rotationally symmetrical quartz glass crucibles
US20040118156A1 (en) * 2001-03-08 2004-06-24 Gabriele Korus Method of producing a quartz glass crucible
CN1323964C (zh) * 2002-08-15 2007-07-04 日本超精石英株式会社 石英玻璃坩埚的重整方法
US20100055222A1 (en) * 2008-08-30 2010-03-04 Japan Super Quartz Corporation Apparatus for the production of silica crucible
US20100154701A1 (en) * 2008-12-19 2010-06-24 Heraeus Shin-Etsu America, Inc. Silica crucible with pure and bubble free inner crucible layer and method of making the same
US20110123738A1 (en) * 2009-11-20 2011-05-26 Heraeus Shin-Etsu America, Inc. Method of making a silica crucible in a controlled atmosphere
US20110198336A1 (en) * 2010-02-12 2011-08-18 Masahiro Hoshino Apparatus for purifying metallurgical silicon for solar cells
US8501140B2 (en) 2010-07-21 2013-08-06 Masahiro Hoshino Method and apparatus for purifying metallurgical silicon for solar cells
TWI406825B (zh) * 2009-10-02 2013-09-01 Japan Super Quartz Corp 氧化矽玻璃坩堝的製造裝置以及製造方法
US8673073B2 (en) 2009-11-16 2014-03-18 Masahiro Hoshino Methods for purifying metallurgical silicon
CN111683906A (zh) * 2018-02-06 2020-09-18 信越石英株式会社 碳电极及石英玻璃坩埚的制造方法

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JP4300333B2 (ja) * 2002-03-14 2009-07-22 ジャパンスーパークォーツ株式会社 リング状アークによる石英ガラスルツボの製造方法と装置およびその石英ガラスルツボ

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US7350378B2 (en) * 2000-07-11 2008-04-01 Heraeus Quarzglas Gmbh & Co. Kg Method for producing rotationally symmetrical quartz glass crucibles
US7797966B2 (en) 2000-12-29 2010-09-21 Single Crystal Technologies, Inc. Hot substrate deposition of fused silica
US20020083741A1 (en) * 2000-12-29 2002-07-04 Pandelisev Kiril A. Hot substrate deposition of fused silica
US20040118156A1 (en) * 2001-03-08 2004-06-24 Gabriele Korus Method of producing a quartz glass crucible
US6755049B2 (en) * 2001-03-08 2004-06-29 Heraeus Quarzglas Gmbh & Co. Kg Method of producing a quartz glass crucible
US20020139143A1 (en) * 2001-03-08 2002-10-03 Gabriele Korus Method of producing a quartz glass crucible
CN1323964C (zh) * 2002-08-15 2007-07-04 日本超精石英株式会社 石英玻璃坩埚的重整方法
US20100055222A1 (en) * 2008-08-30 2010-03-04 Japan Super Quartz Corporation Apparatus for the production of silica crucible
US8075689B2 (en) * 2008-08-30 2011-12-13 Japan Super Quartz Corporation Apparatus for the production of silica crucible
US20100154701A1 (en) * 2008-12-19 2010-06-24 Heraeus Shin-Etsu America, Inc. Silica crucible with pure and bubble free inner crucible layer and method of making the same
US8272234B2 (en) 2008-12-19 2012-09-25 Heraeus Shin-Etsu America, Inc. Silica crucible with pure and bubble free inner crucible layer and method of making the same
TWI406825B (zh) * 2009-10-02 2013-09-01 Japan Super Quartz Corp 氧化矽玻璃坩堝的製造裝置以及製造方法
US8673073B2 (en) 2009-11-16 2014-03-18 Masahiro Hoshino Methods for purifying metallurgical silicon
US20110123738A1 (en) * 2009-11-20 2011-05-26 Heraeus Shin-Etsu America, Inc. Method of making a silica crucible in a controlled atmosphere
US9003832B2 (en) 2009-11-20 2015-04-14 Heraeus Shin-Etsu America, Inc. Method of making a silica crucible in a controlled atmosphere
US8461487B2 (en) * 2010-02-12 2013-06-11 Masahiro Hoshino Apparatus for purifying metallurgical silicon for solar cells
US8524188B2 (en) 2010-02-12 2013-09-03 Masahiro Hoshino Method for purifying metallurgical silicon for solar cells
US20110198336A1 (en) * 2010-02-12 2011-08-18 Masahiro Hoshino Apparatus for purifying metallurgical silicon for solar cells
US8501140B2 (en) 2010-07-21 2013-08-06 Masahiro Hoshino Method and apparatus for purifying metallurgical silicon for solar cells
CN111683906A (zh) * 2018-02-06 2020-09-18 信越石英株式会社 碳电极及石英玻璃坩埚的制造方法

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